RESEARCH ARTICLE Challenges and Advances in Development of Active Components to Modify Headspace Gases in Packaging of Fresh Produce and Muscle Foods PREFACE API 2015

Ziynet Boz Bruce A. Welt* University of Florida University of Florida

Jeffrey K. Brecht William Pelletier University of Florida University of Florida

Eric McLamore Greg Kiker University of Florida University of Florida

Jason E. Butler University of Florida

ABSTRACT

Modified Atmosphere Packaging (MAP) has been widely used as an effective way to preserve foods. Fresh produce, meat and meat products, seafood, and dairy products can benefit from modified gaseous atmospheres, which are usually achieved by reducing oxygen and increasing carbon dioxide concentrations, within limits, defined by product tolerances. MAP of fresh produce is particularly challenging because products are living and respiring. Respiration rates depend on several factors including temperature, oxygen, and carbon dioxide concentrations. Balancing package permeation with respiration is challenging, often due to limited selection of practical packaging materials. Failing to remain within tolerance limits of products leads to rapid quality loss. Gas barrier properties of packages determined rate of gas exchange with the external environment and is a critical factor for achieving tolerable levels. Availability of packaging materials that meet requirement of specific produce is essential. Relative permeability of common films to carbon dioxide is about 3 to 6 times of that to oxygen, often leading to package collapse for package atmospheres that benefit from carbon dioxide. Films often fail to provide desired oxygen transmission rates, high carbon dioxide to oxygen selectivity and desired mechanical properties simultaneously. Despite advances, minimal availability and high cost of selective barrier films limit applications of MAP for fresh produce packaging. Therefore, active packaging components and films are being developed and designed to overcome these limitations. Inserts or films that contain active mixtures as gas emitters

Challenges and Advances in Development of Active Components 62 RESEARCH ARTICLE and/or scavengers are now commercially available. “Clean label” trends are motivating alternative approaches using active packaging components.

KEY WORDS

modified atmosphere packaging, MAP, food, muscle, fresh, produce, respiring, respiration, active packaging

PREFACE API 2015 *Bruce A. Welt Corresponding Author [email protected]

INTRODUCTION ergonomic and aesthetic designs. Technologies such as active and intelligent packaging have been The food industry has been shaped by changing proposed, but have not yet been fully realized com- consumer demands and availability of a wide variety mercially [7]. Modified atmosphere packaging of foods. Past decades have witnessed the increased (MAP) can provide benefits by slowing deteriora- consumption of products with proven advantages tive reactions. Sales volumes of advanced packag- to human health and well-being. Fruits and veg- ing technologies and MAP continue to grow and etables were demonstrated to have health benefits are anticipated to reach $6.4 billion by 2020 [8]. against chronic disease and cancer [1]. Fish and One of the most challenging aspects of MAP is the lean red meats provide essential macro and micro- unique atmospheric requirements for the variety of nutrients [2], [3]. Muscle food products remain the products. In red meats, oxygen is necessary for the main source of protein and nutrients [4]. Accel- bright red color expected by consumers, but oxygen erating consumption of fresh produce, meat and also contributes to degradative oxidation. There- fish has led to improved post-harvest/post-mortem fore, techniques to control oxygen exposure are of handling, processing, packaging, transportation, value to red meat products. Respiring fresh produce and retail practices. However, the perishable and require distinct levels of oxygen and carbon dioxide. variable aspect of natural, high-value products con- Typically, oxygen levels lower than atmospheric tinues to challenge industry to develop methods to and carbon dioxide higher than atmospheric are preserve “freshness” without compromising safety. needed. Great care is required to ensure that oxygen Improved preservation could mitigate loss of nearly is not reduced to levels that result in anaerobic res- one-third of foods produced [5]. Recent consumer piration. For fish, the primary goal of MAP is pre- preferences for minimally processed foods and venting microbial growth. Relatively high carbon overall “freshness” have led marketing efforts to dioxide levels help to reduce pH via equilibrium switch focus from “shelf life extension” to “pres- of the dissolved gas with carbonic acid. Therefore, ervation of preferred quality” Although shelf life is flushing packages with carbon dioxide as high as an important parameter, the main selling factor is 100% by volume may prove useful [9]. quality as perceived by the consumers [6]. Elevated carbon dioxide concentrations are Packaging innovations have been mainly often desirable in packaged foods anti-microbial limited to barrier modifications as well as improved effects, regardless of product type. Carbon dioxide is

Journal of Applied Packaging Research 63 soluble in aqueous solutions, food tissues and packag- The European Commission Regulation (EC) ing materials. Rate of permeation of carbon dioxide No 450/2009 on active packaging defines active through polymers is three to seven times greater than materials as “Materials and articles that are for oxygen [10]–[12]. A comprehensive review on O2/ intended to extend the shelf-life or to maintain or

CO2 diffusivity and solubility in a variety of foods and improve the condition of packaged food; they are polymers was written by Chaix et al. [13]. designed to deliberately incorporate components Loss of gas from packages combined with sol- that would release or absorb substances into or ubility of headspace gases in packaged products from the packaged food or the environment sur- causes reductions in volume in flexible packaging, rounding the food can aid overcoming product- resulting in unattractive, deflated packages that may specific challenges”. Thus, active packaging is con- appear to be less than “fresh” [10], [14]–[16]. Defla- sidered a secondary level of packaging, but may tion [17] causes misconceptions about defects related play a role in primary functions, such as modified to products and/or packaging, such as inferior pack- atmosphere [19]. Gas emitting or scavenging via aging materials or methods, microbiological activity active components comprises a significant portion or seal defects. Industry recognizes package volume of active packaging. Adjustment of package gas changes as a problem and works to mitigate the requires knowledge of effects on biochemical pro- problem by adjusting initial volumes of headspace cesses, physical interactions, microbial flora [20], gases and by considering shipping distances [18]. and other variabilities. MAP and AP applications Understanding the distinct atmospheric may be justified based upon value-added consumer requirements of foods drives research, process- convenience, new product opportunities that did not ing and packaging innovation. MAP advances otherwise exist, branding opportunities, extended have been realized in mathematical modeling and maintenance of quality, reduced waste, and/or computer simulation, materials development and higher margins. Increasingly, due to regulatory properties analysis and measurement and gas gen- and/or consumer preference, chemical preserva- eration, mixing and handling. Modified package tives cannot be added in certain foods or package atmospheres may be obtained actively or passively. materials. For this reason, vacuum packaging, due “Active” MAP involves injection of the desired to its simplicity and effectiveness, remains partic- atmosphere into packages so as to instantly arrive ularly important [21]. For example, a recent trend at the targeted atmosphere. “Passive” MAP relies of “clean-label” products creates an opportunity for upon interactions among product (e.g. product res- food preservation through MAP and AP by elimi- piration rate), package (i.e. gas transmission rates) nating artificial food-additives [22]. and the environment (i.e. ambient gas composition and temperature) to arrive at target atmospheres MAP AND PRODUCT CONSIDER- sometime after packaging. Often, optimal modified ATIONS atmospheres cannot be attained using commercially available packaging materials and/or gas flushing. For example, due to differences in permeation rates Map Considerations for Fresh Produce of gases, we may be able to achieve the desired level Biological activity in fresh produce continues for oxygen or carbon dioxide, but not both at the after detachment from the plant. Harvested produce same time. Additionally, carbon dioxide emitters draws resources from its own stores causing degra- may be used to prevent package collapse. dation. Deterioration rate is influenced by respiration

Challenges and Advances in Development of Active Components 64 rate, ethylene sensitivity and exposure, genetics, Oxygen serves as final electron acceptor in physical injuries, microbiological activity and physi- aerobic respiration reactions [35]. The typical goal ological disorders [23]. Generally, reduction of respi- of MAP is to reduce oxygen to the lowest possible ration rate is the primary objective of MAP for fresh level that supports aerobic respiration. When oxygen produce. Respiration is a primary process for con- levels drop below this threshold, anaerobic respira- sumption of reserves of carbohydrates, lipids, and tion ensues, which rapidly diminishes quality. Use proteins. Depletion of nutrient resources and build-up of other gases to promote quality retention, such as of reaction by-products manifests as decreasing fresh- nitric and nitrous oxides, Sulphur dioxide, chlorine, ness. Pectolytic enzyme activity causes changes in ozone and propylene oxide have been used for a texture and aroma. Such changes are often associated variety of reasons [36], [37]. Economic benefits and with the rapid ripening processes referred to as senes- consumer value should be considered before imple- cence [24]. Enzyme mediated metabolic rates are menting MAP for a given product [38]. affected by variety, harvesting time and processing Use of oxygen-enriched atmosphere (super- conditions [25], [26]. MAP has been reported to help atmospheric oxygen) has also been studied for to preserve firmness of dried apricots and table grapes making produce less susceptible to thermal abuse. [27], [28]. Slowing metabolic activity with reduced Degree of benefit appears to vary with commod- oxygen and elevated carbon dioxide preserves fresh- ity, maturity and ripeness [39]. Escalona et at. ness [29]. However, benefits to texture and aroma [40] reported that super-atmospheric oxygen was depend on type of produce and specific MAP condi- only beneficial when used with moderate levels of tions such as minimum and maximum tolerable O2 carbon dioxide. More work is needed to assess the and CO2 concentrations. Taking MAP beyond toler- value of super-atmospheric gas concentrations in able limits of produce results in increased softening MAP applications. and off-flavor development. Consumers distinguish subtle differences in aroma and texture associated Effect of Intrinsic Properties and Processing with freshness so care must be taken to understand Variations in respiration rate are inevitable and MAP design as well as environmental aspects of the due to both extrinsic and intrinsic factors. Intrin- supply chain [30]–[32]. sic factors include variety, maturity, composition, and size. Typically, ±10% deviation in respiration Gas Concentrations rate are observed in separate batches of the same Understanding factors that cause variations in produce [41]. Seefeldt, Løkke, and Edelenbos [26] respiration rate is important for MAP design. Equi- observed respiration rate differences in produce librium atmospheres should be within a “window” harvested in early versus late summer as well as of optimum gas concentrations for different produce differences among four broccoli varieties. Respira- [33]. Gas concentrations in packages depend on tion rate differences due to variety have been shown package gas transmission rates (GTR), respiration to be as large as 60% among three MAP packaged rate of produce, respiration quotient (carbon dioxide apricot varieties [25]. Such variations make design- molecules liberated per oxygen molecule consumed) ing MAP challenging. and ambient conditions. When the partial pressure of Cutting, wound formation and mechanical oxygen decreases within a package due to respiration injury tend to cause respiration rates to increase, or oxidative reactions, permeation of oxygen into the leading to accelerated ethylene production, water package, from the environment increases [34]. loss, texture and color changes and increased

Journal of Applied Packaging Research 65 microbiological activity [42]. Therefore, respiration on L. monocytogenes [51], [52]. Physiochemical rates of fresh-cut commodities tend to be higher composition of products, such as low pH, repre- than intact produce. Heat treatments also cause res- sents a hurdle for certain bacteria in foods, which piration rate differences depending on pre-harvest can lead to proliferation of acid tolerant spoilage condition and exposure duration. Postharvest heat bacteria, yeasts, and molds. treatments are gaining attention due to reductions Vegetables are susceptible to growth of patho- of respiratory and microbial activity and preven- gens and spoilage microorganisms, which may be tion of chilling injury [43]. Changes in respiration suppressed by MAP. Due to competition, spoilage rate and quality were studied during heat treatment bacteria tend to limit pathogenic microorganisms in combination with MAP of several commodi- [53] causing food to spoil before becoming toxic. ties including, asparagus, tomatoes and fresh cut Concerns related to MAP of fresh produce are due melons [44]–[46]. A review of research on the com- to microorganisms that survive at cold storage tem- bination of minimal processing and MAP was pre- peratures (i.e. psychrotropic L. monocytogenes, sented by [47]. Table 1 summarizes recent research Yersinia enterocolitica and Aeromonas hydrophila) of processing conditions on respiration rate. Com- and under anaerobic or low oxygen (fermentative) bining varieties in packages (i.e. salad mixes and conditions such as Salmonella, E. coli O157:H7 fruit platters) has become popular. Since differ- and L. monocytogenes [54]. Clostridium botulinum ent varieties exhibit different respiration rates and is always a safety concern in low-acid foods (pH typically require different gaseous atmospheres for >4.6) due to possible liberation of deadly boltuli- optimal preservation of freshness, compromises in num neurotoxin under anaerobic conditions [55]. package design must be made. Typically, packages Under chilled and modified atmosphere conditions, are designed to accommodate the highest respira- growth of pathogens suppresses growth of indige- tion rate ingredient. nous microflora such asPseudomonas spp. Entero- bacter spp. and lactic acid bacteria [51], [56]. Microbial Consequences Samonella causes the most illness among all Data from 2004 to 2013 show that the fresh pathogens in fresh produce [48]. Salmonella and produce is the primary source of outbreaks that facultative anaerobes are capable of growing with caused human illness [48]. MAP conditions influ- and without oxygen. Low oxygen conditions may ence microflora differently based on complex inter- promote growth of pathogens initially present on actions with produce and environmental conditions produce. Horev et al. [56] and V. Rodov et al. [57] in the supply chain [49]. Highly soluble CO2 offers demonstrated that Active MAP favored growth of antimicrobial activity but can damage produce Salmonella enterica in romaine lettuce whereas tissue at high concentrations. Although the specific passive MAP had no apparent effect except for functioning mechanism is not known, suggested reductions in total bacterial counts. Vegetables at theories focus on the replacement of O2 for the bac- abusive temperatures promote growth of patho- terial activity, reduction of pH, direct penetration gens [58]. Abusive temperatures have been demon- into the cell and intracellular liquid , and direct/ strated to increase the number of pathogens such as indirect inclusion of CO2 in the metabolic reac- E. coli 0157:H7, Salmonella and L. monocytogenes tions [50]. Also, CO2 may not inhibit certain robust in MAP produce [52], [59], [60]. pathogens. Elevated carbon dioxide concentrations Spoilage microorganisms play an important (changing from 5% to 12%) had no inhibitory effect safety role by causing detectable spoilage before

Challenges and Advances in Development of Active Components 66 pathogens liberate toxins [36], [61], [62]. However, gas composition and form of packaging [87]. High spoilage may not always occur prior to pathogen postmortem water activity (0.65-0.8), pH (>6) and growth. Aesthetic quality and consumer accept- non-protein nitrogen compounds render fish and ability did not change for MAP stored butternut fish products susceptible to the microbial spoilage, squash and onions even after liberation and detec- although changes in sensory characteristics usually tion of botulinum toxin for products stored under appear before the spoilage occurs [88]. different temperatures including o 5 C [63]. Simi- larly, botulinum toxin appeared in ultraviolet radi- Meat Products ation treated fresh-cut cantaloupes and honeydew Meat quality is characterized by its color, water melons before visual quality changes were holding capacity/exudate, microbial activity and observed at 15oC [62]. Hintlian and Hotchkiss, [62] lipid composition [89], [90]. Consumers are mostly developed the “Safety Index,” which represents influenced by color. Discoloration causes economic the ratio of spoilage microorganisms to pathogens, loses [91]. Color changes can also induce other which helps to predict likelihood of spoilage prior deteriorative reactions. For example, interaction of to danger from pathogens before consumption. The meat discoloration and lipid autoxidation in a ran- major challenge is assessment of food safety by cidity producing catalytic cycle has been shown considering these complex microbial interactions [92]. Changes in red color of meat by oxidation are under MAP and cold storage throughout the supply promoted by the ferrous associated blood protein, chain. Recent studies published on microbiological myoglobin. Oxidation of myoglobin is promoted by aspects of atmosphere modification demonstrate a variety of factors including increasing tempera- effects of vegetable and packaging type, varying tures and light exposure [93]. In this process, oxy- gas concentrations and temperatures on growth and genation of purple deoxymyoglobin forms red oxy- survival of several pathogens [52], [56], [57], [65]– myoglobin, which may be oxidized to form brown [67]. Extensive reviews on microbiological aspects metmyoglobin [91]. Brown colored metmyoglobin of MAP in fresh and fresh-cut produce have also formation from deoxymyoglobin is not desired in been available [14], [36], [49], [55], [58], [68]. fresh red meat, therefore its formation is delayed by keeping myoglobin in the deoxygenated pur- Map Considerations For Muscle Foods and ple-color form via MAP, Vacuum Packaging (VP), Products Vacuum Skin Packaging (VSP) and active packag- Preparation and packaging of muscle products ing (AP) technologies. transitioned from separate, in-store operations Protecting deoxymyoglobin from oxygen is to centralized processing facilities using con- achieved by combining high and low barrier packag- sumer-ready packages. This has paved the way ing films with vacuum and/or oxygen-free gas. For for implementation of MAP technologies [85]. retail display, high oxygen barrier film is removed, MAP is among the most convenient technologies exposing a high oxygen transmission layer, causing to maintain and extend the shelf life of muscle meat to “bloom” red. This approach is referred to products without food additives [86]. Similar to “master-packs,” and “tray-in-sleeve.” Trays, lidding fresh produce, extending the shelf life of fish by films, master-pack barrier films, Vacuum Skin atmosphere modification depends on the nature of Packaging (VSP) trays made of materials with high product such as fat content and microbial flora and oxygen barrier such as polyvinylidene chloride load, and external factors including temperature, (PVDC) or polyethylene vinyl alcohol copolymer

Journal of Applied Packaging Research 67 Table 1: Recent literature on assessment of intrinsic and extrinsic factors on respiration rate and different parameters of fresh and fresh-cut produce.

yi to Biooi ete oe eeene to UV-C processing effects NA RR, microbial growth, Red Oak Leaf lettuce [69] sensory and quality (Lactca sativa L.) parameters Temperature, packaging films NA RR, color variation Iceberg and Romaine lettuce [70] Electron-beam irradiation NA RR, microbial growth, Fresh-cut cantaloupes (Ccmis melo [71] sensory and quality Linnaeus, cv. Magellan and Acclaim) parameters

Temperature, MAP storage time, NA RR, RQ, Ea Carrots (Dacs caota L.) [72] cutting type

Temperature, transient O2 and NA RR Green banana (sa paadisiaca L) [73]

CO2 concentration changes

Temperature, O2, CO2 Biological RR, RQ Agaics mushrooms [38] composition

Gelatin coating, Temperature NA RR, RQ, Ea minimally processed organic carrots [74] (Dacs caota L. cv. Brasília)

Ar, He, N2, O2 in combination NA RR, ethylene production, Aragula salad (ca vesicaia Mill.) [75] with two sanitation treatments storage time, quality parameters, bioactive compounds color, microbial quality Temperature Variety, RR Broccoli species (assica oleacea, [26] Harvest Time Italica Group) and Wild Rocket Salad Diplotais tenifolia L.) Cut size, blade-sharpness, Origin, RR Fresh-cut pineapple (MD2) [76] dipping process physiological age, seasonality Temperature, MAP NA RR, RQ, quality Fresh cut apple (als domestica [77] parameters oh) CV Gala Temperature Seasonal Ethylene production, Plums, (ns domestica L.) [78] variations, RR, RQ Maturity state

O2, CO2, storage time Harvest time, Off odors, RR, ethanol, Fresh-cut iceberg lettuce [79] Maturity stage, acetaldehyde, weight, (Lactca sativa L.) Cultivar, edge browning Volatiles

Critical O2, low temperature NA RQ, RR, chilling injury Cucumbers (Ccmis sativs L.) [80]

storage, CO2 absorber

Cold plasma treatment and O2, NA RR, microbial reduction, Strawberries [81]

CO2, N2 mixtures quality parameters Changing mixing proportions of Overall RR, Ethylene Fresh-cut pineapple, apple and [82] the produce production melon mixtures Packaging types and NA RR, quality parameters, Green chillies (Capsicm annm L.) [83] corresponding MAP environment physiological loss Active MAP, Passive MAP NA RR, sensory and quality Pomegranate arils (cv. Wonderful) [84] parameters, physio- chemical parameters, microbial quality Temperature (Heat treatment), NA RR, visual quality, Fresh Cut Melons (Ccmis melo L.) [46] Active MAP decay development

eitoy otient eition te tition ney ot ie

Challenges and Advances in Development of Active Components 68 (EVOH) nylon, as well as high oxygen transmitters (10-30%). Despite extended shelf life, carbon such as polypropylene, polystyrene and polyethyl- dioxide tolerant lactic acid bacteria produce acidic ene are used in MAP of meat. Red meat products off-flavors and aromas, representing the main not suitable for immediate sale, such as primal-cut, cause of spoilage in vacuum packaged products. ground beef are stored in atmospheres with less Typical concentrations for MAP of packaged meat than 0.1% oxygen [94]. are 10-40% and 60-90% carbon dioxide. Due to For shelf-ready products, MAP is usually bacteriostatic effects, 100% carbon dioxide may achieved with elevated oxygen and carbon dioxide be used [98]. High carbon dioxide levels result in [95]. On the other hand, high oxygen MAP can also package collapse through permeation and dissolv- cause color degradation. Super-atmospheric oxygen ing in products. Product to gas ratios should at in MAP affected color stability by triggering oxida- least be equal to two and dissolved gas should be tion and myoglobin oxidation in chilled fresh beef compensated for with excess amounts of gas [99], [96]. Color stability can be improved by low levels which can be provided by gas emitters. In a recent of carbon monoxide (CO), which binds to myoglo- study, a gas mixture containing the highest carbon bin preferentially to, protecting the molecule from dioxide ratio tested (20:50:30% of O2:CO2:N2) oxidation. Carbon monoxide treatment stabilizes showed the most inhibitory effects on Enterobac- color to such an extent that it can also be disadvan- teriaceae in minced meat containing pork and beef tageous because uncooked color may persist even [100]. Detailed microbiological aspects of meat and after cooking. The “fresh” uncooked appearance poultry products can be found in [101]. may also hide indications of spoilage. Venturini et al. [97] assessed optimal anoxic gas mixtures on Fish Products microbial, color and sensory attributes of fresh beef Quality degradation in fish and fish products muscles and concluded an optimal mixture of 39.8% may stem from microbial spoilage, enzyme activity, and lipid oxidation. Microbial spoilers responsible N2, 60% CO2 and 0.2% CO for maintaining color without growth of L. monocytogenes or S. aureus. from degradation in texture, flavor and appearance in seafood include Pseudomonas spp., Shewanella In another study 99.6% CO2 and 0.4% CO mixture enabled growth of Listeria species in master-pack- putrefaciens, Photobacterium phosphoperum, Vib- aged pork while preserving the color quality. rionaceae and Enterobacteriaceae. These microbes Aerobic storage of meat facilitates fast-grow- are referred to as seafood specific spoilage organisms ing microflora Pseudomonas, Psychrobacter and (SSO) and represent only a small portion of initial Moraxella [98]. Spoilage often originates on product microflora present. Conditions such as gas compo- surfaces by aerobic microorganisms resulting in sition, temperature, high water content and addi- decomposition of proteins such as collagen with tives such as sodium chloride (NaCl), create selec- consequent production of proteinaceous slime and tive environments promoting growth of SSO relative off-odors [95]. Shelf life extension is achieved by to the broader population of microflora. SSO growth limiting aerobic, Gram-negative microorganisms to leads to off-flavors limiting shelf life of fish. Trimeth- promote Gram-positive and slow growing microor- ylamine (TMA) is a key contributor to fishy odors. ganisms such as lactic acid bacteria and Micrococ- Low molecular weight off-flavors such as hydrogen caceae. Vacuum packaging, when combined with sulfide (H2S) and other sulfur compounds, ammonia, muscle-based chemical reactions can create low biogenic amines, acetic acid and hypoxanthine con- oxygen and elevated carbon dioxide concentrations tribute to spoiled aroma [102]. TMA is produced from

Journal of Applied Packaging Research 69 trimethylamine oxide (TMAO) primarily through this problem. Above certain concentrations, dis- the action of trimethylamine oxidase enzyme from solved carbon dioxide creates a carbonated “fizzy” spoilage bacteria, which can even be produced under mouthfeel for cooked and raw fish. Fletcher et al. chilled and oxygen-free conditions. This reaction [108] developed a model to correlate product to is responsible for fish spoiling relatively faster than gas ratio and carbonated flavors in fresh salmon. other muscle foods [103]. MAP has the capacity to They found the optimum ratio of 0.5-1 mL carbon increase shelf life by inhibiting growth of SSO as well dioxide per gram of product. as limiting the lipid oxidation. Since dissolved carbon dioxide forms an There are several criteria when selecting equilibrium with carbonic acid, which reduces optimal gas concentrations in MAP for fish and fish pH, carbon dioxide may denature water-holding products. Skura [104], [9] reviewed MAP in fish proteins resulting in increased drip-losses [9]. and fish products including cod, salmon, haddock, Fish packaged under MAP or vacuum in pre-rigor catfish, tilapia, swordfish, snapper, herring, shrimp is more susceptible to increased drip losses as and trout. The typical approach was minimizing compared to fish packaged in post-rigor [109]. Even oxygen and increasing carbon dioxide to 60-100%, though benefits of MAP often exceed drawbacks, exploiting antimicrobial effects of carbon dioxide. one risk associated with MAP in fish is growth of Due to high solubility of carbon dioxide in toxin producing anaerobic pathogens at oxygen organic materials such as polymer packaging films concentrations lower than 4-8%. The primary and tissues of the packaged products, initial head- pathogen of concern is the obligate anaerobe Clos- space volumes and concentrations cannot be pre- tridium botulinum. Inclusion of oxygen should be served throughout the shelf life without a source able to prevent toxin production [110]. Additionally, of new gas. Carbon dioxide emitters represent a response of anaerobes can vary in fish. Addition of relatively new active component for packaging in oxygen does not necessarily guarantee elimination order to stabilize soluble gases. This are referred of risk of botulism. Maintaining cold chain tem- to as soluble gas stabilization (SGS). However, peratures (<3.5oC) from harvest to retail prevents even after opening a package enriched with carbon growth of C. botulinum [111]. L. monocytogenes, dioxide, residual gas was shown to be sufficient to Yersinia enterocolitica and Aeromonas spp. are suppress spoilage microflora and provide for addi- also pathogens of concern at low temperature and tional shelf life [105]–[107]. Due to Henry’s law, oxygen conditions. Typically, increasing carbon headspace gas seeks equilibrium with gas dis- dioxide concentrations leads to delayed toxin pro- solved in products. Equilibrium concentrations duction. Higher carbon dioxide levels represents of dissolved gas depend upon partial pressure of one possible hurdle among a number of hurdles gas in the headspace and product composition. (e.g. temperature, preservatives, water activity, As headspace gas dissolves in products, flexible etc.) that together protect consumers from patho- packages deflate. Product to gas ratio should be at gens [110]. Regulators such as FDA, prefer that least 2:1 to 3:1 by volume for effective microbial spoilage bacteria grow unimpeded so that products preservation and maintenance of package integrity present clearly as spoiled before toxin is produced. [9]. However, increased headspaces lead to higher In an imprecise world, there is always a risk of toxin package volumes, which consume precious volume production before spoilage. Therefore, temperature within the supply chain. Carbon dioxide emitters control is the most essential factor in ensuring food and soluble gas stabilization techniques mitigate safety with and without MAP or AP.

Challenges and Advances in Development of Active Components 70 Temperature control validation can be done Poultry Products with smart packaging technologies such as time- MAP has been shown to be able to double shelf temperature integrators (TTI) [9]. Food safety life of poultry products [117]. However, literature verification can be done by coupling the response related to poultry MAP is limited. Since microbial reaction of the TTI’s with practically meaningful spoilage is the primary concern, elevated carbon properties, such as initiation point for the toxin dioxide concentrations have been applied. Typical production. However, many end-point indicators carbon dioxide concentrations vary between are rather “programmed” to respond to tempera- 40-100% by volume balanced with nitrogen [118]. ture kinetics directly. Welt et al. [112] designed Under anaerobic conditions, Pseudomonas spp. can an improved performance TTI to adjust responses be suppressed, however, acid tolerant anaerobic according to a well-known empirical relation- and facultative microorganisms such as lactic acid ship presented by [113]. The same principle can be bacteria and Enterobacteriaceae cause spoilage applied to design novel TTIs including effects of via slime and off-odors [119]. Meredith et al. [118] other definitive parameters for an increased selec- demonstrated shelf life extension benefits using tion based on product type. For example, Gunvig 40:30:30% (CO2:O2:N2) on Campylobacter, 50% et. al. [114] developed a model to predict growth of and 70% of carbon dioxide on lactic acid bacteria C. botulinum with changing external conditions of and Pseudomonas, respectively. High oxygen con- temperature, pH, NaCl, sodium nitrite and sodium centration MAP in turkey breast has shown slightly lactate in meat products. better retention of color and sensory characteristics Reduction of quality through autolytic enzymes than low oxygen concentrations [120]. and chemical reactions begins immediately after harvest and manifest even before evidence of dete- Importance of External Factors rioration due to microbial growth. Oxidation of Reducing temperature and oxygen levels reduces polyunsaturated fatty acids is the main concern for reaction rates that use oxygen, such as aerobic res- non-microbial spoilage in fish. Changes in flavor, piration in fresh produce. Among these, temperature odor and color caused by such reactions leads to is the most important external factor [15]. Tempera- reductions in shelf life and sales [115]. High-fat fish ture does not only influence respiration rate, but vir- such as salmon, herring and cod are more suscep- tually all reactions that influence safety and quality. tible to oxidation. Therefore, oxygen is removed Gas transmission rates of package materials and sol- through vacuum or MAP with elevated carbon ubility of gases in packaged products are also influ- dioxide and balanced with nitrogen to help mitigate enced by temperature. Ideally, storage temperature oxidation in such products, but oxygen perme- should be kept at the lowest level that does not cause ation into packages results in persistent residual chill damage for the purpose of slowing reactions as levels. Oxygen scavengers have been shown to much as possible. Maintaining temperature through be capable of reducing headspace oxygen to less the supply chain is often referred to as the “cold than 0.1% from atmospheric concentrations [116]. chain management,” and it involves temperature Antioxidant compounds have been incorporated control during handling, transportation, distribution in packaging materials in combination with MAP and retail [65]. Mathematical models used to design for a variety of products. Table 2 shows synergis- MAP assume exposure to specific temperatures. tic effects of MAP with other preservation methods Deviations from assumed temperatures cause devia- for muscle products. tions in packages and when excessive, may result in

Journal of Applied Packaging Research 71 Table 2: Examples of recent studies on combination of MAP and hurdles. ot ition e e eeene onenttion Ready to use peeled MAP Thymol essential oil 9 days of shelf life increase when MAP and [121] shrimp thymol combined. MAP alone or thyme oil at high concentration could not provide shelf life extension. Bluefin tuna fillets N2 flushing α-tocopherol Reduced lipid and hemoglobin oxidation [122] Pacific white shrimp 75:10:15% Controlled freezing point Shelf life extended to 11- 12 days. [123] o (CO2:O2:N2) temperature (-0.8 C)

Gilthead se bream 5:95% (O2:CO2) Grape fruit seed extract, Extended microbial and sensory qualities for [85] thymol, chitosan 8-10 and 20 days, respectively. Catfish slices 35:5:60% Tannic acid Reduced lipid oxidation and suppressed [124]

(CO2:O2:N2) growth of psychrophilic and mesophilic bacteria

Poultry sausages 100% CO2 High Hydrostatic Pressure When combined with 100% CO2, lower [125] pressures can be used for inactivation of L canosm themosphacta L innoca

Ground beef 20:80% (CO2:O2) Tannic acid Better color stability, psychrophilic bacteria [126] and limited lipid stability were obtained with

incorporation of tannic acid in high O2 MAP Beef Varying mixtures Clove oil, cinnamon oil, Patent that claims a shelf life increase up to [127] illicium verum oil 24 days undesirable and/or unsafe conditions. For respiring purposes and human interactions. Business prac- produce, predicted equilibrium/steady-state gas con- tices cause extra storage days at distribution centers centrations in MAP packages can only be expected and wholesale markets under non-optimum condi- when products are stored within assumed temper- tions, which leads to decreased shelf life, especially ature ranges. Tano et al. [128] studied atmosphere for delicate, temperature-sensitive crops like bananas, and quality changes of mushrooms, broccoli and cucumbers and tomatoes [131]. Therefore, many labo- tomatoes under abusive temperatures and reported ratory experiments and recommendations based on that fluctuating temperatures promoted anaerobic optimum temperature conditions fail to reflect the “non- respiration, resulting in off-flavors, ethanol and acet- optimal” shelf life realized commercially [132]. Slight aldehyde development. They also showed that anaer- temperature deviations cause a stronger response on obic conditions develop based on the highest tem- respiration rates than packaging gas transmission rates perature reached and headspace of the package. [15], [26]. Understanding practical ranges of conditions Though controlled, temperature is rarely constant is helpful to successful design of MAP. A common throughout the cold chain [129]. Ninety percent of approach adopted to select the appropriate temperature produce that benefit in relatively low temperatures is the “approximate achievable temperature,” which is (<4oC) encounter retail temperatures higher than the calculated by considering optimum and prospective recommended. Moreover, deviations from optimum abusive temperatures in the calculations. For example, storage temperatures vary with seasonal changes by as if the produce has the optimum storage temperature of much as 87% and 93% in summer and winter, respec- 0oC and the highest expected temperature abuse during tively [130]. Distribution centers and retail outlets cause handling and display in the supermarket of 15oC, the most temperature abuse due to convenience, marketing approximate average of these temperatures (7oC) is

Challenges and Advances in Development of Active Components 72 chosen as the basis. This approach may fail to achieve losses for the sellers [42] since produce is mostly desired equilibrium concentrations in packages. sold by weight. Packaging films tend to trap water Microbial and non-microbial spoilage are tem- vapor in packages, which may be mitigated with perature-dependent, therefore temperature is the anti-fogging polymer additives and/or perforations. most important factor to control muscle foods as However, perforated films do not have the same gas/ well [9]. Even psychrophilic bacteria (i.e. Pseudo- vapor transmission characteristics as non-perforated monas spp.) have a reduced growth rate at tempera- films [137]. Resistance to transfer of water vapor in tures below 10oC [9]. Solubility of carbon dioxide perforated packaging depends on the number and increases with decreased temperatures, which can size of perforations [134]. However, increasing the be advantageous due to its pH lowering bacterio- number and/or size of perforations leads to loss of static effects or disadvantageous regarding package benefits related to MAP. Industry has been devel- collapse. Dual-function carbon dioxide emitters, oping solutions for monitoring environmental con- such as citric acid and sodium bicarbonate contain- ditions during cold chain operations. Recent devel- ing absorbent pads may be useful [133]. opments include advancements in time temperature Temperature fluctuations also affect relative indicators/integrators (TTI’s) including programma- humidity (RH%). Storage studies are often per- ble digital TTI’s, smart labels and enhanced commu- formed without RH% control, especially at high nication systems with cloud based storage and real- RH% conditions where most of the fresh produce is time alerts with smart phone applications. Figure stored [132]. However, at low temperature storage, 1 shows indicators that can monitor the tempera- even slight temperature differences can cause large ture abuse as well as time spent at those conditions. swings in RH%. When temperatures fall below dew In timestrip® TTI’s, two migration mediums are points water condenses on colder surfaces. Result- brought in contact with rupture activation to produce ing availability of liquid water facilitates microbial a color change as a function of temperature. Table 3 growth and related spoilage [134]. This can be miti- shows a summary of related commercial solutions. gated by sufficient aeration during storage, but that Fresh produce packaged with transparent films is mostly effective for unpackaged produce. Linke are exposed to varying light conditions in the supply and Geyer [135] investigated condensation inten- chain. Proper lighting in retail displays is impor- sity under changing temperature conditions of tant for consumer perception. In addition to other packaged plums and demonstrated that in-package metabolic activities, photosynthesis plays a role in and produce condensation is separately affected by gas composition changes for green and leafy veg- environmental air flow, amplitude of the varying etables due to presence of chlorophyll. Quality of temperature, package headspace and cycle time. baby spinach was reported to increase when stored Lower RH% values cause accelerated moisture and under low light conditions along with increases in associated weight loss of products, as well as losses carbon dioxide. Increasing light intensity tends to in firmness, texture, and color. Open storage appli- reduced quality such as leaking of solutes from cations are relatively easier to control by mechani- leaves and declines in ascorbic acid [138]. Baby cal systems. Packaging films typically do not have spinach stored under MA conditions caused less cell adequate water vapor transmission rate (WVTR), damage with varying light conditions [139]. Mar- resulting in condensation and unsightly fogging tínez-Sánchez et al. [140] demonstrated reductions on the inner layer of the package [136]. Reduction of browning and increase in visual quality of cut of water from packages translates into economic romaine lettuce under dark conditions. However,

Journal of Applied Packaging Research 73 due to the development of high carbon dioxide and by photooxidation of lipids [141]. Light was found low oxygen concentrations, anaerobic respiration to be destructive to color in cooked and sliced ham,

was triggered in their samples. Higher permeability however, and color was more stable in 30% CO2 and

films were recommended for low light conditions. 70% N2 MAP packages [142]. Beef and ham were shown to be affected negatively

Fig. 1: Finger-pressure activated time indicators timestrip® PLUS ™ and timestrip® for displaying the time elapsed at the specified temperature threshold (Timestrip UK Ltd.).

Table 3: Summary of the commercial products to display temperature and humidity deviations for fresh produce storage and packaging. oei e ntion ein eie ony UltraContact and Ultra Wireless Smart labels with temperature sensors with the Ultra Contact or PakSense Inc. Labels option of real time monitoring of the ambient or Wireless surface temperatures Thinfilm Smart Label Printed label with programmable upper and lower NA Thin Film and PST limits of the allowable temperatures and indicates Sensor exceeded limit on the label Monitor Mark® Time Temperature Indicator (TTI) with NA 3M information on exposure time

Tectrol® Check Sticker MAP Pallet Indicator for berries with a switch of NA Trans Fresh and Insignia color when accumulation of time exceeds the Technologies critical limit at abuse temperatures. RF Wireless Temperature Sensors Placing the sensors in different locations and food Wireless FreshLoc Technologies simulators in refrigerated systems and real time Inc. communications on cloud based sharing. ThermoTrace TTI Label for Temperature control Laser Scanner DeltaTrak® Inc.

sense® HiTags RF Sensor Tags for real time temperature and RH Wireles BT9 Ltd. control and Cold Chain Logistics evaluations and communication cloud based data from producer to retail end user units Timestrip® TTI Label for monitoring temperatures customized NA TimeStrip® for varying thresholds from 3oC-10oC up to 4 hours of abuse conditions. Fresh Check® TTI Label for Consumer Use NA TempTime Corporation

Not Available

Challenges and Advances in Development of Active Components 74 ACTIVE PACKAGING COMPONENTS complex and costly film technologies. Due to TO MEDIATE MODIFIED ATMO- increasing consumer demand for high quality SPHERES and minimally processed foods, global revenue of oxygen scavengers including sachets, films and Modified atmospheres can be supported or facil- food products are expected to reach $2.5 billion by itated through scavengers, emitters, and integral 2020 with a five year compounded annual growth components of packaging materials. Depending on rate of 3.1% [8]. The purpose of oxygen scaven- specific requirements of products, active packag- gers is to minimize product exposure to oxygen ing (AP) systems are designed to emit, scavenge, that is initially dissolved as well as oxygen that or maintain gas and/or vapor (e.g. moisture, aroma). enters packages via permeation, diffusion and Active components are provided in a variety of leaks. Oxygen scavengers have been shown to be forms including sachets, sheets, film coatings, capable of reducing residual levels to less than closure liners or embedded in package materi- 0.01%, (Rooney, 1995b). Oxygen scavengers use als as laminates. Committing to use active compo- a variety of agents including iron, enzymes (i.e. nents leads to concerns related to accidental inges- glucose oxidase and alcohol oxidase), photosen- tion by consumers, leaks or release from broken sitive dyes, ascorbic acid and unsaturated fatty inserts into foods and/or failures to add components acids. Effectiveness is defined by overall capacity to packages during manufacture [116]. Regardless and rate of absorption [146]. In iron-based scaven- of the form, moisture-activated active components gers, presence of acids such as malic acid, tartaric will not function if required moisture levels are not acid, acetic acid, potassium bitartrate, alum, reached in packages. Additionally, permeable layers benzoic acid, and citric acid promote accelerated should be aligned with active components to enable oxidation [147]. Additional chemical systems used active exchange with package environments [143]. are Metal/Acid Nylon MXD6, catechol, ferrous The most widely used absorbers can actively modify sulfate, salt-copper sulfate carbonate. Oxygen oxygen, carbon dioxide, ethylene and moisture, acet- scavengers are selected based on cost, packag- aldehyde, sulfide, bitterness, lactose and UV-light ing format, shelf-life extension required, water [144]. One problem related to active compounds is activity of food, initial and required final oxygen their own storage stability, since they are active. levels [20] and storage temperature. This is especially problematic after incorporation The most widely used oxygen scavengers are into film structures [145]. When possible, an ini- individual sachets, inserts, labels or strips contain- tiation mechanism (e.g. U.V. triggered) should be ing iron and/or ferrous salts that are oxidized in the included. Current commercial oxygen, ethylene and presence of moisture, which is typically provided carbon dioxide absorbers/emitters and their use for from moist products. Electron transfer during oxi- packaging is provided in Table 4. dation is accelerated by aqueous solutions and elec- trolytes which is explained by the primary mecha- Gas Absorbers nism of oxidizing iron to ferric oxides and hydrox- Absorbers, when used in combination with ides with the presence of water. Thus, perfor- MAP, enables higher production speeds and better mance of moisture dependent scavengers depends performance than vacuum or gas flushing alone on product water activity and their scavenging [21]. Oxygen scavengers in packaging of muscle rates can be adjusted for specific %RH condi- foods offers potential to reduce dependency on tions. For example, for dry products, water must be

Journal of Applied Packaging Research 75 introduced to activate the scavenger. [144] reported Ethylene is a growth and maturation hormone that iron containing labels should not be used with in plants and can be removed from fresh produce acidic foods (e.g. tomato sauce) where rapid iron packages by absorbers containing active ethylene- migration may exceed the maximum tolerable limit oxidizing reactants. Commonly used scavengers of 48 mg per kg of food. Iron migration is negligi- are in forms of sachets and polymer films con- ble for dry and low water activity foods. However, taining potassium permanganate. Potassium per- films should be separated from food contact to manganate is first oxidized to acetaldehyde and minimize migration [148]. Sachet-type absorbers then to acetic acid. When there is enough potas- are often packaged in a separate paper-polyethyl- sium permanganate, carbon dioxide and hydrogen ene packages. While iron-based oxygen scaven- are produced, and intermediate reactants, such as gers are safe, it is difficult to determine whether potassium hydroxide, are formed irreversibly. sachets are fresh or have already been depleted. Sachet contents appear black when fresh and red Gas Emitters (i.e. rusty) when depleted [149]. Carbon dioxide emitting systems usually

Use of enzymes are challenging due to temper- include dual function (i.e. simultaneous O2 scaveng- ature and pH sensitivity, aqueous medium required ing and CO2 emitting). Especially for products such and price. Alcohol oxidase does not require water as fresh produce benefiting from high CO2 levels, and is suitable for low water activity products, but required high permeability films to maintain a although storage stability may be affected when certain level of O2 to prevent anoxia. CO2 emitters embedded in polymer [150]. This is due to the include sodium bicarbonate, fumaric acid, calcium sensitivity of enzymes to pH, temperature, water chloride, fumed silica [152], ascorbic acid, citric presence. There are methods to increase storage acid and ferrous carbonate. Metal halides generate stability of enzymes in the polymeric matrix such carbon dioxide when exposed to water. A novel, as preserving the water monolayer around the moisture initiated O2 emitting and CO2 absorbing embedded enzymes, immobilization to solid struc- technology was awarded a patent by the United ture and reduced mobility with increased glass Kingdom, which includes a mixture containing transition temperatures. However, immobilization carbonate peroxyhydrate component placed in O2 has disadvantages like reduced enzyme activity per permeable laminate pouch [153]. Such technology volume of film and higher costs [151] Sulfite salts can be included in packages designed for super- can also be used to reduce oxygen while produc- atmospheric O2 packages, to keep the O2 concen- ing sulfates. Such organic-based active substances trations at beneficial higher levels due to 2O lost via including ascorbic acid, unsaturated fatty acids and package permeation. enzymes do not interfere with metal detectors on Multi-Function Absorbers and Emitters production lines. Due to sensitivity of some fresh produce to carbon dioxide its accumulation from Muscle foods and high carbon dioxide tolerat- product respiration can be reduced using absorb- ing fresh produce require elevated carbon dioxide ers. Components used for absorbing carbon dioxide and lower oxygen, which can lead to package defla- include calcium hydroxide (involving water depen- tion. Exudates and/or condensed water may need dent absorption to produce calcium carbonate), to be removed in order to avoid formation of envi- sodium hydroxide, potassium hydroxide, calcium ronments favorable for microorganisms. Multiple oxide and adsorption on silica gel. function absorbers/emitters serve these purposes.

Challenges and Advances in Development of Active Components 76 For example, a moisture activated mixture of sodium emitters also serve for color stability, postharvest bicarbonate, fumaric acid, sodium erythorbate, ripening for green-picked climacteric produce ferrous sulfate, calcium chloride and fumed silica and antimicrobial purposes. Due to their toxicity, is contained in absorbent and microporous layers release of such chemicals should be controlled. absorbing oxygen and exudates while releasing carbon dioxide [143]. Calcium hydroxide and iron Active Absorbers and Emitters in Fresh powder are combined to absorb oxygen and carbon Produce and Muscle Foods dioxide [154]. Dual function ethylene and oxygen Fresh Produce absorbers are effective in limiting microbial growth and reducing respiration rate [155]. Figure 2 illus- Oxygen, carbon dioxide and ethylene absorb- ers in fresh produce were shown to be effective trates a multi-function CO2 emitter and moisture absorber active pad application for salmon. in preventing color and texture changes caused by non-enzymatic reactions. Charles et al. [157] dem- Other Absorbers and Emitters onstrated use of a commercially available, iron- based oxygen absorber (ATCO® LH100, Standa Moisture absorbers Industies, France) in tomatoes packaged in low Due to high moisture of fresh produce and fresh density polyethylene (LDPE) film, helped to reduce muscle foods, condensation is often an issue under time required to reach optimal oxygen concentra- variable temperature conditions [21]. Exudates are tions, which limited respiration rate and prevented controlled via absorbent pads, pouches, or mats. excess carbon dioxide production. Charles et al. Condensation is mitigated by anti-fogging addi- [158] demonstrated a reduced transitional period tives in polymers, but these promote droplet for- of 50 versus 100 hours with the reduced iron- mation, which then drip downward in packages. based oxygen scavenger (ATCO® LH-100) and The most common moisture absorbing/adsorb- with carbon dioxide absorber containing sodium ing agents are silica gel, propylene glycol, polyvi- hydroxide (ATCO® CO-450). Charles et al. [159] nyl alcohol, modified starch, clay etc. [21], [111], observed a delayed greening and browning with [156]. Polyacrylate salts and copolymers grafted by the LDPE packages with LH-100 oxygen scav- starch are examples of commonly used polymers engers on fresh endives compared to the micro- [21]. Ethylene, sulfur dioxide and chlorine dioxide perforated Oriented Propylene (OPP) and LDPE

Lidding film

Tray

AbsorbentActive Pad

Fig. 2: Multi-function active pads with exudate capturing and CO2 emitting capabilities to provide prolonged shelf life for muscle products.

Journal of Applied Packaging Research 77 Table 4: Commercial gas regulating AP components used in fresh produce and muscle foods.

ye ony oei ne ntion o ot e Ageless® type ZP and ZPT Iron powder oxidation Ageless® type SS Fast reacting type, self-reacting Dried meats, beef jerky, Mitsubishi Gas Chemical Co., ® Ageless type GLS Organic non-iron type suitable for metal detectors. processed meats, Japan Ageless® type F-L Water dependent (initiated) iron oxidation fish, and seafood Ageless® OMAC® Iron-based film for aseptic and retort processing applications Standa Industrues, France Distr. Meat, fish, poultry and ATCO® Iron powder oxidation, iron-based labels with by Emco Packaging Systems, UK seafood products. Iron powder oxidation sachet Toppan Printing Co., Japan Freshlizer Ascorbic acid oxidation Multilayer polymer with ethylene methyl acrylate, Chevron Phillips OSP® Wet and dry food cyclohexane methyl acrylate FreshPax® Iron powder oxidation sachets ® Multisorb Technologies Inc., FreshCard Multifunctional O2 absorbing cards Sliced meats, smoked USA ® and cured meats JerkyFresh O2 absorbing packets and strips ® Fresh Max O2 absorbing adhesive labels O-BUSTER® (imported Iron powder oxidation by absorbing packets and Processed and dried meats Desiccare, Inc., USA from Taiwan) strips IRON FREE® Non-iron type Processed and dried meats Pillsburry Co., USA OxySorb® Multilayer polymer film Sealed Air Corp. (Cryovac Div.), Dried or smoked meat ®

Absorbers Cryovac OS 2000 Multilayer polymer activated by ionizing radiation

2 USA products, processed meats O Tea, tomato products, Diamond Clear® Plastipak Packaging Inc. PET resins for containers and bottles vitamin enhanced products Shelfplus® O , Shelfplus® Albis Plastic, Germany 2 Oxygen absorbing film and high barrier film O2 3200 Clairant International, OYGUARD Sachets Processed meat Switzerland Dried fruits and nuts, Amelco Dessicants Inc. H Type, S Type, P Type Sachets bakery products, snacks Oxygen scavenging closure sealant and CELO® 210, 210B, PET and bottle GCP Applied technologies masterbatch, non-PVC scavengers with polyolefins 210W, 300, 2002, 2003 applications fo MAP foods with aw>0.65 Nutricepts, Inc. OxyVac® Enzyme based oxygen scavenger and cheeseproducts Drypak DryPak Oxygen Absrober Oxygen absorbing sachets Dry and solid foods Active carbon and oxygen absorbing component Dried laver, sardines, ham, TOMATSU® contained in green tea. Suitable for metal detectors confectionery

OhE Chemicals, Inc., Japan SEQUL Iron-based scavenger Confectioneries, dried fish Apples, Japanese pears, CRISPER HF Ethylene absorbing sachets persimmons,kiwi, broccoli, melon

Standa Industrues, France and Products with CO ATCO®CO Carbon dioxide absorber bags 2 Emco Packaging Systems, UK 2 sensitivity Absorbers 2 CO

Challenges and Advances in Development of Active Components 78 Table 4 cont’d: Commercial gas regulating AP components used in fresh produce and muscle foods.

ye ony oei ne ntion o ot e Produce retail bags containing minerals and Peakfresh®, USA Fresh produce and flowers household-type sachets Produce retail bags containing minerals, sachets

Evert-fresh Corporation, USA Evert-Fresh Green Bags containing minerals for ethylene and CO2 Fresh produce and flowers absorption IMPAK Corporation, USA epax Ethylene absorbing sachets Fresh produce and flowers

Ethylene Absorbers Sealed Air Corp. (Cryovac Div.), Dri-Loc® Moisture absorbing pads, oven-safe and compost- Fresh produce and fresh USA able absorbent meat pads, pouches and mats meat, fish, poultry Varying RH% from 32% to 84%. Each package Dried fruits, popcorn, ® ® has various salt solutions for appropriate humidity Boveda , Inc., USA Boveda conditions. E.g. 84% RH includes water, xanthan sugar, spices and herbs, gum, potassium chloride and potassium sorbate tobacco, herbal medicine Fresh meat, fish, poultry, Sirane Ltd., UK Dri-Fresh® Moisture absorbing pads and liners fresh produce including asparagus and berries Dual-compartment vacuum pack to separate SEALPAC® TenderPac® Fresh meat exudates

Maxwell Chase Technologies, ® Fresh-cut fruits and

Moisture Absorbers Fresh-R-Pax Absorbent trays and pads LLC vegetables MacAirlaid Inc. MeatGuard Absorbent pads with superabsorbent fibers Fresh meat, fish, poultry Mitsubishi Gas Chemical Co., Preventing the package shrinkage by O absorbing Ageless® type GE 2 Rice cakes, nuts, dried fish Japan and CO2 emitting Moisture dependent and self-reaction type oxygen Freund Corporation, Japan Negamold® absorbers, controlling the yeast and stilis by ethanol vapor. Super-atmospheric O Emco Packaging Systems, UK OxyFresh® O emitting with CO scavenging technology 2 2 2 packaging of fresh produce Fresh whole, divided, ® Nutricepts, Inc. OxyVac -S Enzyme based O2 scavenger and CO2 emitter. cooked muscle foods (aw>0.65)

® Coffee and products that Ageless type E O2 and CO2 scavenging sachets are sensitive to O2 and CO2 Solution for package Mitsubishi Gas Chemical Co., shrinking in several Japan ® Ageless type GT O2 absorbing and CO2 emitting sachets products e.g. fresh and processed meat, poultry, fish and fresh produce Persimmons, bamboo OhE Chemicals, Inc., Japan CRISPER NK Carbon dioxide and moisture absorbing sachets shoots, kiwi fruit, citrus fruits and pickles

Moisture absorber, CO2 and antimicrobial emitter Fresh meat and poultry, Paper Pak Industries UltraZap® tenda Pak containing citric and sorbic acid mixtures in form fresh cut produce of cellulose pads (e.g. fresh cut tomatoes)

Multiple Function Absorbers and Emitters Multiple Function Strawberries, tomatoes, broccoli, washed lettuce Citric acid and sodium bicarbonate containing ® and muscle foods Co2 Technologies CO2 Fresh Pads moisture absorbent and CO emitter pads 2 including meat, seafood, fish and poultry. CO emitting polymer material with carbonates or CSP Technologies Activ-Pak 2 Bottles and cap liners bicarbonates CO emitting, fluid absorbing system embedded Vartdal Plastindustri AS SUPERFRESH 2 Salmon, Cod, Chicken into the bottom tray.

Journal of Applied Packaging Research 79 packages without scavengers. Jayathunge and absorber. They showed labels manufactured from Illeperuma [160] analyzed color, percent weight active biofilm could preserve quality of shiitake loss, ethanol and carbon dioxide production and mushrooms for five days by preventing moisture consumption of oxygen of oyster mushrooms and carbon dioxide accumulation in packages. packaged with varying amounts of magnesium oxide as carbon dioxide scavenger. They dem- Muscle Foods onstrated increased shelf life from 6 to 12 days. Carbon dioxide emitters prepared with sodium A carbon dioxide absorber based on sodium car- bicarbonate and citric acid mixtures contained in bonate peroxyhydrate, sodium carbonate, sodium moisture absorbent pads were demonstrated to be chloride and bentonite clay mixed in two dif- more effective in increasing shelf life and reducing ferent combinations (EMCO-A and EMCO-B, headspace to product ratio than vacuum packag- EMCO Packaging Systems, UK) were shown to ing of pre-rigor fillets and loins of Atlantic cod be effective in preserving quality of strawberries [166], [167] and Atlantic salmon [168]. Packages by maintaining equilibrium carbon dioxide levels with oxygen absorbers or carbon dioxide emitters in packages [161]. An ethylene absorber based limited growth of L. monocytogenes, Enterobac- on palladium chloride and charcoal was dem- teriaceae and total aerobic bacteria in ready-to-eat onstrated to be beneficial for limiting ethylene meat product, whereas antimicrobial compound, exposure and texture loses in kiwifruits, bananas allyl isothiocyanate, was only effective onL. mono- and chlorophyll degradation in spinach leaves cytogenes [169]. Carbon dioxide emitters included [162]. Home-use ethylene absorbing bags incor- in chicken fillet packages were shown to be ben- porating sodium permanganate (Blueapple®, eficial in extending shelf life and decreasing drip Aureus Products Innovations Inc., UT, USA), and losses caused by high carbon dioxide storage, potassium permanganate with zeolite (ExtraL- however, package collapse was observed [170]. ife®, Dennis Green Ltd., CO, USA). [163], evalu- Essential oils and natural antioxidants are some- ated carbon dioxide absorbing characteristics of times used as reducing agents to prevent oxidation four chemicals including calcium oxide, magne- in muscle food products. Inclusion of oregano oil in sium hydroxide, sodium carbonate and calcium combination with iron-based absorbing sachets were hydroxide in high density polyethylene sachets shown to increase shelf life of rainbow trout fillets of kimchi. They demonstrated enhanced carbon from 4 days to 17 days via microbial and sensory dioxide absorption rate when sodium carbonate analyses [171]. Rosemary extract was found to be and zeolite were combined in active sachet film. more efficient than a commercial oxygen scaven- [164] developed a moisture regulating tray with ger in preventing High Pressure Processing (HPP)- sodium chloride and ionomer mixed as a hygro- induced lipid oxidation in pork patties [172]. Sirocchi scopic active layer and determined absorption et al. [173] demonstrated 15-day increased shelf life kinetics in different salt solutions, and separately of refrigerated beef when stored at high oxygen con- in tomatoes and strawberries. They demonstrated centrations in packages containing active polyeth- effectiveness of trays with 12% by weight NaCl in ylene sheets sprayed with rosemary essential oil. tomatoes, however, moisture loss in strawberries Emitters can include chemicals and natural compo- was observed. Wang et al. [165] developed an agar nents to release oxygen, carbon dioxide, nitrogen, based biofilm as sodium carbonate and sodium ethylene, antioxidant, antimicrobials, sulfur dioxide, glycinate as active moisture and carbon dioxide chlorine dioxide and flavor [144].

Challenges and Advances in Development of Active Components 80 ADVANCEMENTS AND FUTURE or void spaces that are resistant to the diffusion). WORK Scales in multiscale modeling can be at various levels. For example, Defraeye et al. [178] inves- tigated effects of micro parameters (i.e. surface Mathematical Modeling Approach cracks, lenticels and water droplets) on gas and Estimation of gas concentration changes with heat exchange dynamics of apples (i.e. convec- different package and produce parameters is nec- tive heat and mass transfer coefficients) in a essary before a successful MAP application can microscale computational fluid dynamics (CFD) be designed. The “Pack and Pray” approach rarely modeling approach, where they also assessed achieves desired outcomes [174]. Mathematical modeling parameters. CFD at single scale is also models combined with computer simulation can an efficient tool to predict dynamic changes with predict transient and equilibrium gas composi- various conditions in MAP. Bonis et al. [179] used tions as they are affected by mass transfer (i.e. dif- CFD to predict average temperatures and oxygen fusion, gas and water vapor permeation through and carbon dioxide concentrations in the package the package material and plant tissue), physio- headspace coupled with microbiological load and chemical reactions due to the plant metabolism moisture distributions for the MAP truffles and (i.e. respiration, transpiration) and heat transfer cactus pears. No literature was found on multiple (i.e. external cooling and internal heat genera- scale models focusing on gas releasing/absorbing tion by the produce respiration). For food pack- AP components. Predictive gas kinetics of AP- aging, the majority of these models are based on mediated MAP were studied by [158], [180]–[182]. macroscopic balances. Increasing computational Parameter uncertainties through interval analysis power has led to improved models that help us were modeled in fresh produce package design to understand the complex mechanisms and bio- [183], for which applications can be expanded. chemical processes occurring in MAP products. Structures at smaller scale such as cells and inter- Trends and Challenges cellular spaces are responsible for macro-level Adopting recent active packaging technology changes such as gas exchange. Therefore, multi- depends on economics, preferences of producers, scale modeling may prove to be useful in MAP. retailers and consumers. Particularly, costs related Multiscale modeling has recently been applied to to advanced packaging methods and correspond- postharvest research in attempts to relate macro- ing willingness by consumers to pay a premium scopic attributes such as diffusion parameters to or to realize cost savings from these technologies microscopic structures [175]. Ho et al. [176], [177] that offset investments are required. Moreover, evaluated gas exchange mechanisms by diffusion consumer viewpoints for enhanced quality via pack- laws and calculated diffusion coefficients as well aging is limited [184]. Packaging materials should as partial pressure differences of carbon dioxide be developed to meet the functions of a packag- and oxygen using 2D pear and 3D intact apple ing system and should be able to inform consumers micro-structures. They found that variations in about the product contents such as nutritional values gas permeation values are caused by distributions [185]. Regional differences play an important role. of micro structures and selectivity of gas diffusion For example, the North American market is more (i.e. different paths for oxygen and carbon dioxide) “consumer/packer” oriented, whereas the European through these structures (i.e. intracellular liquid market is determined mainly by retailers [186].

Journal of Applied Packaging Research 81 The use of bio-based and biodegradable mate- food packaging applications was recently patented rials in active as well as passive packaging has been [198]. A multilayer oxygen absorbing film contain- gaining popularity over the recent years. Scarfato ing a scavenging layer of ethylene/methyl acrylate/ et al. [187] demonstrated a biodegradable oxygen cyclohexene methyl acrylate copolymer (EMCM) scavenger with alpha-tocopherol and poly(lactic) was also recently patented [199]. acid (PLA) formulation. Pant et al. [188] developed Besides benefits, there are challenges to a bio-based oxygen scavenging film with extrusion consider when designing MAP with active pack- and lamination of bio-based layers of adhesive, aging. Chemical-containing active packaging may Gallic acid and sodium carbonate mixture as the have the disadvantage of rejection by health-con- active layer, a food contact layer, and PLA. Junior scious, natural product-oriented consumers, espe- et al. [189] developed a linear low density polyeth- cially when used as external parts such as pouches ylene-starch based film with increased biodegrad- or sachets. Accidental ingestion or rupture of the ability, which was incorporated with citric acid to sachets are among the primary concerns [200], provide active packaging properties in beef pack- [201]. Hence, recent efforts to incorporate active aging. Similarly Stoll et al. [190] demonstrated the components into package films are becoming effect of starch based film incorporated with anti- popular in order to reduce interactions of active oxidants from wine grape pomace on the quality of components with consumers [19]. extra virgin olive oil. Domenek et al. [191] inves- tigated the antioxidant and mechanical properties of biodegradable PLA-lignin films. Even though consumer preference towards bio-based materials increase, there are drawbacks associated with PLA films, poor barrier properties for 2O , CO2 and N2 [192], and high costs [193]. Active and intelligent packaging patents associ- ated with meat packaging from early 2000’s to 2014 were reviewed by [194]. Some recent patents are also included in this section. Novel approaches include incorporation of active agents into the packaging film, maintaining refrigerated temperatures and improvements to existing package configurations. A recent patent was issued for an oxygen emitter for meat packaging [195] that involves a single layer film incorporating an iron-based oxygen scaven- ger and a moisture regulating agent that functions at refrigerated temperatures [196]. Another patent involves a potassium permanganate/polymer blend that can absorb oxygen and ethylene produced by fresh produce [197]. N-hydroxyimide derivates and transition oxygen scavenger metals such as cobalt, nickel or copper in transparent polyolefin films for

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